Thin films of multiwalled carbon nanotubes/polyaniline nanocomposites (CNT/PAni) were synthesized through the liquid/liquid (L/L) interfacial route, deposited over glass substrates, and evaluated through cyclic voltammetry and amperometry as electrochemical sensor, using L-ascorbic acid as probe. Films with three different CNT/PAni ratios have been prepared. After the spectroscopic and morphological characterization, the electrochemical sensitivity towards L-ascorbic acid was evaluated and compared with similar sensors prepared from neat multiwalled carbon nanotubes (MWCNT) or neat polyaniline (PAni). The nanocomposite film that presented the best nanotube dispersion through the polymeric matrix presented the higher sensor sensibility, 0.237 µA (µmol L−1)−1 and a limit of detection (LOD) of 7.91 µmol L−1. These results evidenced a synergistic effect among the components, and the best response depended on strict control of the polyaniline matrix distribution surrounding the nanotubes.

Biochar is a rich-carbon material highly functionalized, which allows the use as electrodes modifier for preconcentration and voltammetric determination of several species. This work describes a castor cake biochar production and chemical activation with different reaction conditions using HNO3 and/or H2O2. Biochar samples were characterized using scanning electron microscopy, energy dispersive spectroscopy, thermogravimetric analysis, Fourier-transform infrared spectroscopy, Raman and zeta potential. Carbon paste modified electrodes (CPME) have been constructed using different biochar samples to evaluate the adsorptive capacity for the spontaneous preconcentration and voltammetric determination of Pb2+, Cd2+, Cu2+ and Ni2+ ions, paraquat and methyl parathion pesticides. The activation treatments promoted modifications in the elemental, morphological and structural biochar characteristics. Activated biochar CPMEs showed increase in the current signal around 15 and 2.5 times higher than unmodified and precursor biochar electrode, respectively. N2 sample (HNO3, 60 °C for 3.0 h) presented the better response signals for all compounds. This was attributed to the more effective surface oxidation, promoting a high porosity, acid character and amount of acid functional groups. Besides that, this greater analytical response allows the CPME-N2 application as a passive sampler for the voltammetric determination of inorganic and organic contaminants for environmental management in aqueous matrices.

O presente trabalho reporta o desenvolvimento de um novo método voltamétrico para análise de íons ouro(III) usando eletrodo de carbono impresso modificado com poli-L-histidina. O procedimento é baseado no acúmulo do complexo [AuCl4]-, na superfície do eletrodo sob potencial de circuito aberto e tempo de acúmulo controlado. Parâmetros que influenciam na resposta, tais como: preparação do filme, pH, potencial de acúmulo e tempo de acúmulo, foram otimizados e curvas analíticas para os íons ouro foram construídas usando voltametria de varredura linear (LSV), pulso diferencial (DPV), e onda quadrada (SWV). Limites de detecção de 6,0 × 10-6 mol L-1, 1,7 × 10-6 mol L-1 e 4,0 × 10-6 mol L-1 foram obtidos para LSV, DPV e SWV, respectivamente. O método foi aplicado para a determinação de íons ouro em amostras de urina humana.

A sensitive voltammetric method for trace measurements of gold(III) ions using a screen-printed carbon electrode modified with poly-L-histidine is described. The new procedure is based on the accumulation of the tetrachloroaurates complex at the electrode surface under an open circuit potential condition, followed by a cathodic stripping scan of potential. Parameters such as film preparation, pH, accumulation potential and deposition time have been optimized to obtain the best voltammetric response. Using optimal experimental conditions, analytical curves for gold ions were obtained using a linear sweep (LSV), differential pulse (DPV), and square wave voltammetry (SWV). Limits of detection of 6.0 × 10-6 mol L-1, 1.7 × 10-6 mol L-1 and 4.0 × 10-6 mol L-1 were estimated for the LSV, DPV and SWV, respectively. The method was successfully applied to the determination of gold ions in human urine samples.